Quantitative analysis equipment for active pharmaceutical ingredients

Abstract

The invention relates to the technical field of pharmaceutical analysis equipment, and discloses pharmaceutical active component quantitative analysis equipment which comprises a chromatographic column, the chromatographic column comprises a hollow column body, a filter screen is fixedly arranged at the lower end in the column body, a stationary phase is arranged above the filter screen, a piston is arranged above the stationary phase, and the piston is connected with a driving part; the piston comprises a first shell facing the stationary phase, a second shell is coaxially arranged on the side, away from the stationary phase, of the first shell in a sliding mode, an elastic supporting piece is arranged between the first shell and the second shell, a plurality of connecting holes are coaxially formed in the bottom of the first shell and the bottom of the second shell, liquid discharging columns are arranged in the connecting holes, and liquid inlets are formed in the tops of the liquid discharging columns. A liquid outlet is formed in the side wall of the bottom of each liquid discharging column, the multiple liquid discharging columns are connected with a driving mechanism, and the second shell is connected with a liquid inlet pipe. According to the invention, the state of a stationary phase bed layer can be actively adjusted, and uniform introduction and dispersion of liquid medicine are realized, so that the chromatographic separation efficiency and the quantitative analysis accuracy are improved.

Description

Technical Field

[0001] This invention relates to the field of pharmaceutical analysis equipment technology, and in particular to a quantitative analysis device for active pharmaceutical ingredients. Background Technology

[0002] Chromatography is one of the core technologies in modern pharmaceutical analysis used for the separation, purification, and quantitative analysis of complex mixtures. Its basic principle is based on the difference in partition coefficients between the stationary and mobile phases of the sample. When the two phases move relative to each other, the components undergo multiple partitions between them, thus achieving separation. The chromatographic column, as the heart of the chromatographic system, directly determines the separation efficiency, resolution, and reproducibility through the performance and packing state of the stationary phase (such as silica gel or bonded phases) it contains.

[0003] In the quantitative analysis of active pharmaceutical ingredients, especially when processing samples with complex compositions, high viscosity, or the potential presence of trace particulate matter, such as extracts of traditional Chinese medicine and biological samples, traditional chromatographic columns may experience voids or uneven compaction of the stationary phase bed due to impact from the mobile phase during prolonged operation or under high pressure. Secondly, the initial uniformity of the drug distribution at the column head is crucial. Uneven distribution leads to inconsistent migration rates of sample components across the stationary phase cross-section, affecting peak shape and quantitative accuracy. Conventional injection methods often rely on the natural diffusion of the mobile phase to distribute the sample at the column head, which is ineffective for samples that are difficult to diffuse or have strong adsorption properties. Furthermore, existing equipment typically introduces samples and delivers the mobile phase outside the column, lacking active and controllable means of regulating the state of the stationary phase within the column; the entire separation process passively depends on an external pumping system.

[0004] Therefore, there is an urgent need for a device for quantitative analysis of active pharmaceutical ingredients to solve the above problems. Summary of the Invention

[0005] The purpose of this invention is to provide a device for quantitative analysis of active pharmaceutical ingredients. By setting a piston, the device can actively adjust the state of the stationary phase bed during the analysis process and achieve uniform introduction and dispersion of the drug solution, thereby improving the efficiency of chromatographic separation and the accuracy of quantitative analysis.

[0006] The above-mentioned technical objective of the present invention is achieved through the following technical solution:

[0007] A device for quantitative analysis of active pharmaceutical ingredients includes a chromatographic column. The chromatographic column comprises a hollow column body. A filter screen is fixedly disposed at the lower end of the column body. A stationary phase is disposed above the filter screen. A piston is disposed above the stationary phase. The piston is connected to a driving member that drives it to reciprocate along the axis of the column body. The piston includes a first housing facing the stationary phase. The sidewall of the first housing is slidably sealed to the inner wall of the column body. A second housing is slidably disposed coaxially with the side of the first housing away from the stationary phase. An elastic support member is disposed between the first housing and the second housing. Multiple openings are coaxially formed at the bottom of the first housing and the second housing. A connecting hole is provided, in which a drain column is provided. The drain column is rotatably connected to the second housing. The top of the drain column is provided with a liquid inlet, and the bottom side wall of the drain column is provided with a liquid outlet. A communication channel is provided between the liquid outlet and the liquid inlet. In its natural state, the height of the liquid outlet is higher than the bottom surface of the first housing. When the first housing compresses the fixed phase, the height of the liquid outlet is lower than the bottom surface of the first housing. Multiple drain columns are connected to a driving mechanism, which drives the drain columns to rotate. The second housing is connected to a liquid inlet pipe for delivering the drug solution into the second housing.

[0008] As a further feature of the present invention, the driving mechanism includes a power component and a transmission component. The transmission component includes a first gear that is coaxially and fixedly connected to the drain column. Multiple first gears are meshed with each other. When one of the first gears rotates, it synchronously drives the other first gears to rotate. A first gear is meshed with a second gear. The second gear is rotatably connected to the second housing. The second gear is coaxially connected to a transmission shaft. The power component is connected to the transmission shaft to drive its rotation.

[0009] As a further feature of the present invention, the power component includes a mounting housing fixedly connected to the second housing, the mounting housing having a mounting cavity inside, a first hydraulic gear and a second hydraulic gear being rotatably connected in the mounting cavity, the mounting housing being connected to the inlet pipe on one side of the mounting cavity, and an outlet pipe being connected to the other side of the mounting cavity.

[0010] As a further feature of the present invention, a baffle is fixedly disposed above the first gear and the second gear in the second housing. The baffle and the second housing form a sealed chamber. The first gear and the second gear are disposed in the chamber. The upper end of the drain column passes through the baffle, and its upper end is flush with the upper surface of the baffle.

[0011] As a further feature of the present invention, a scraper is fixedly disposed above the baffle on the drive shaft, and the bottom of the scraper abuts against the upper surface of the baffle.

[0012] As a further feature of the present invention, the driving component includes a hydraulic cylinder consisting of a cylinder body and a hydraulic rod, wherein the hydraulic rod is fixedly connected to the second housing.

[0013] As a further feature of the present invention, the hydraulic rod is provided with an installation channel, the inlet pipe is installed in the installation channel and extends out from the upper end of the hydraulic rod, and the end of the inlet pipe extending out of the hydraulic rod is connected to a pumping system via a hose.

[0014] As a further feature of the present invention, the upper edge of the first housing extends inward to form a first limiting edge, which is slidably connected to the second housing, and the bottom of the second housing extends outward to form a second limiting edge, which is slidably connected to the first housing.

[0015] As a further feature of the present invention, the elastic support includes a spring, the spring being parallel to the axis of the second housing and disposed outside the second housing, a plurality of springs being arranged in a circumferential array along the second housing, one end of the spring being fixedly connected to the second housing and the other end being fixedly connected to the first limiting edge.

[0016] As a further feature of the present invention, a drain outlet is provided at the bottom of the column.

[0017] The beneficial effects of this invention are: This invention provides a device for quantitative analysis of active pharmaceutical ingredients. By pressing down the piston through a drive component, the first housing can directly apply uniform axial pressure to the stationary phase, effectively eliminating channeling or voids that may be caused by the impact of the mobile phase, keeping the stationary phase in a tight and uniform packed state, thereby significantly improving the column efficiency and separation reproducibility of the chromatographic column. It is particularly suitable for long-term operation or processing of complex samples.

[0018] When the first housing compresses the stationary phase, it compresses the spring, thereby exposing the outlet of the drain column to the stationary phase for draining. After the draining is completed, the piston rises, and under the action of the spring, the first housing moves down. The first housing can clean the debris on the drain column, ensuring the cleanliness of the drain column.

[0019] In addition, during the drainage process, the first shell squeezes the stationary phase, which in turn squeezes the drainage column. During the operation of this invention, the drainage column rotates, which can effectively prevent the stationary phase from blocking the outlet when stationary, thus effectively improving the drainage efficiency.

[0020] Finally, the piston of the present invention is equipped with a hydraulic motor composed of hydraulic gears. The hydraulic gears are driven to rotate by high-pressure fluid, and the discharge column is driven to rotate by the transmission shaft, the first gear and the second gear. During the rotation of the transmission shaft, the scraper can also be driven to rotate to scrape the medicine liquid, so that the medicine liquid can flow into the discharge column better and avoid excessive residue of medicine liquid. Attached Figure Description

[0021] To more clearly illustrate the technical solutions in the embodiments of the present invention, the accompanying drawings used in the description of the embodiments will be briefly introduced below. Obviously, the accompanying drawings described below are only some embodiments of the present invention. For those skilled in the art, other drawings can be obtained based on these drawings without creative effort.

[0022] Figure 1 This is a schematic diagram of the overall external structure of this embodiment; Figure 2 This is a cross-sectional structural diagram of this embodiment; Figure 3 This is a schematic diagram of the external structure of the piston in this embodiment; Figure 4 This is a schematic diagram of the piston cross-section structure in this embodiment; Figure 5 This is a schematic diagram of the internal structure of the second shell in this embodiment; Figure 6 This is a schematic diagram of the internal structure of the second housing in this embodiment from another perspective; Figure 7 This is a schematic diagram of the cross-sectional structure of the drainage column in this embodiment; Figure 8 This is a cross-sectional view of the power component structure in this embodiment; In the diagram, 1. Chromatographic column, 11. Column body, 12. Filter screen, 13. Stationary phase, 14. Drain port, 2. Piston, 21. First housing, 22. Second housing, 23. Drain column, 24. Inlet, 25. Outlet, 26. First limiting edge, 27. Second limiting edge, 3. Drive component, 31. Hydraulic cylinder, 32. Hydraulic rod, 33. Mounting channel, 4. Drive mechanism, 41. First gear, 42. Second gear, 43. Drive shaft, 44. Mounting housing, 45. First hydraulic gear, 46. Second hydraulic gear, 47. Outlet pipe, 5. Inlet pipe, 61. Baffle, 62. Scraper, 7. Spring. Detailed Implementation

[0023] The technical solution of the present invention will now be clearly and completely described with reference to specific embodiments. Obviously, the described embodiments are merely some, not all, of the embodiments of the present invention. All other embodiments obtained by those skilled in the art based on the embodiments of the present invention without creative effort are within the scope of protection of the present invention.

[0024] A device for quantitative analysis of active pharmaceutical ingredients, reference Figures 1 to 8 It includes a chromatographic column 1, a piston 2 disposed in the chromatographic column 1, and a drive component 3 that drives the piston 2 to move linearly.

[0025] The chromatographic column 1 includes a vertically placed cylindrical hollow column 11. The upper end and lower end of the column 11 are respectively provided with an upper end cap and a lower end cap. The lower end cap is provided with a drain port 14 for collecting the eluent. Inside the column 11, near the bottom, a filter screen 12 with micropores is fixedly installed to support and filter the chromatographic stationary phase 13 above (e.g., C18 reversed-phase silica gel, ion exchange resin, etc.). Above the stationary phase 13, there is a piston 2 that can slide precisely and sealed up and down along the inner wall of the column 11.

[0026] Piston 2 includes a first housing 21 and a second housing 22. The first housing 21 has a concave structure and faces the fixed phase 13. Its sidewall is fitted with a sealing ring to ensure a sliding seal with the inner wall of the piston 11, preventing the liquid medicine from bypassing. The second housing 22 is located above the first housing 21. The upper end of the first housing 21 extends inward to form an annular first limiting edge 26, which slides in engagement with the outer cylindrical surface of the second housing 22. The lower end of the second housing 22 extends outward to form an annular second limiting edge 27, which slides in engagement with the inner cylindrical surface of the first housing 21. Multiple helical compression springs 7, acting as elastic supports, are vertically installed between the first limiting edge 26 and the outer wall of the second housing 22, and are evenly distributed along the circumference of the second housing 22. In its natural state without external force, the elastic force of the springs 7 keeps the first housing 21 in its lowest position relative to the second housing 22.

[0027] The driving component 3 that drives the piston 2 to rise and fall as a whole is the hydraulic cylinder 31 in this embodiment. The hydraulic rod 32 of the hydraulic cylinder 31 extends downward, and its end is fixedly connected to the top center of the second housing 22.

[0028] At the bottom of the first housing 21 and the second housing 22, a series of through-holes are evenly distributed around the circumference. Each hole houses an independently rotatable drainage column 23. The upper end of the drainage column 23 has an inlet 24, and the lower side wall has an outlet 25. Vertical or inclined connecting channels are machined inside to connect the inlet 24 and the outlet 25. A main inlet pipe 5 is connected to the interior of the second housing 22, introducing the medicine solution from the external infusion pump into the inner cavity of the second housing 22. The liquid then enters the connecting channel through the inlet 24 at the top of each drainage column 23, and finally exits from the outlet 25.

[0029] The key to this embodiment lies in the dynamic position design of the outlet 25 of the drain column 23. In its natural state, due to the support of the spring 7, the bottom surface of the first housing 21 is at a lower position, while the outlet 25 of the drain column 23 is higher than this bottom surface. When the hydraulic cylinder 31 drives the piston 2 to press down, the bottom surface of the first housing 21 contacts the fixed phase 13 and is blocked. The second housing 22 continues to descend under the push of the hydraulic rod 32, compressing the spring 7. Since the drain column 23 is rotatably connected to the second housing 22 but does not move relative to the axial direction, its outlet 25 moves down synchronously with the second housing 22, thereby moving down relative to the first housing 21. When the second housing 22 moves down a sufficient distance, the outlet 25 will drop below the bottom surface of the first housing 21, at which point draining can be performed.

[0030] All drainage columns 23 are driven by a drive mechanism 4 to rotate synchronously in the same direction. The drive mechanism 4 includes a transmission component and a power component. The transmission component includes a first gear 41 fixed to the upper end of each drainage column 23. All first gears 41 are located on the same horizontal plane and mesh with each other, forming a synchronous gear system. When one first gear 41 rotates, the other first gears 41 also rotate synchronously. One of the first gears 41 meshes with a second gear 42. The second gear 42 is rotatably mounted on the second housing 22. The second gear 42 is coaxially fixed to the lower end of a vertical drive shaft 43. A baffle 61 is fixedly installed inside the second housing 22. The baffle 61 is located above the gear system. The baffle 61 and the second housing 22 form a sealed gear cavity, isolating the first gears 41 and 42 from the liquid above and any possible contaminants. The upper end of the drainage column 23 passes through the baffle 61 in a sealed manner, and the top end is machined to be a plane flush with the upper surface of the baffle 61. The upper end of the drive shaft 43 extends upward through the baffle 61, and one or more radially protruding scrapers 62 are fixedly installed on the shaft section located above the baffle 61. The bottom of the scraper 62 lightly touches the upper surface of the baffle 61.

[0031] The power unit, used to drive the transmission shaft 43 to rotate, includes a mounting housing 44 fixed to the second housing 22. The mounting housing 44 has an internal mounting cavity containing a pair of meshing first hydraulic gears 45 and second hydraulic gears 46. The mounting housing 44 has an inlet branch pipe and an outlet pipe 47 communicating with the mounting cavity. The inlet branch pipe is connected to the inlet pipe 5 via a pipeline, and the outlet pipe 47 discharges liquid to the surface of the baffle 61 in the second housing 22. When the liquid flows through the mounting cavity, it drives the hydraulic gears to rotate. The first hydraulic gear 45 is coaxially fixedly connected to one end of the transmission shaft 43, thereby converting fluid kinetic energy into rotational mechanical energy, driving the entire gear train and the discharge column 23 to rotate.

[0032] To optimize the layout, an installation channel 33 is formed by drilling through the hydraulic rod 32 of the hydraulic cylinder 31. The inlet pipe 5 is inserted from the top of the hydraulic rod 32, passes through this installation channel 33, and reaches the interior of the second housing 22. Externally, it is connected to the pumping system via a hose.

[0033] The working principle of this embodiment is as follows: During operation, the piston 2 is driven to descend by the hydraulic cylinder 31. After the first housing 21 contacts the fixed phase 13, it generates resistance, while the second housing 22 continues to move down and compresses the spring 7. At the same time, the drain column 23 also gradually descends with the second housing 22 until the outlet 25 of the drain column 23 drops below the bottom surface of the first housing 21.

[0034] Subsequently, the liquid medicine is pumped under high pressure into the inlet pipe 5 through the pumping system, and then enters the mounting cavity through the inlet pipe 5 to impact the first hydraulic gear 45 and the second hydraulic gear 46, causing the two hydraulic gears to rotate. The liquid medicine is discharged from the outlet pipe 47 on the other side of the mounting cavity, enters the interior of the second housing 22, falls onto the baffle 61, and then enters the drain column 23. Since the outlet 25 of the drain column 23 is now below the bottom surface of the first housing 21, the liquid medicine is discharged from the inlet 24 of the drain column 23 through the connecting channel and from the outlet 25 into the fixed phase 13. During the rotation of the first hydraulic gear 45, the transmission shaft 43 is driven to rotate. When the transmission shaft 43 rotates, it drives the second gear 42 to rotate, and simultaneously drives multiple first gears 41 to rotate, thereby driving the drain column 23 to rotate. On the other hand, it drives the scraper 62 to rotate, which allows the liquid medicine on the baffle 61 to better enter each drain column 23.

[0035] After the drainage is completed, cleaning fluid is injected to clean the entire equipment. After cleaning, the piston 2 is moved upward by the hydraulic cylinder 31. When the first housing 21 is separated from the fixed phase 13, the first housing 21 moves downward relative to the second housing 22 under the action of the spring 7. During the downward movement, the side wall of the drainage column 23 can be cleaned.

[0036] By pressing down the piston 2 with the drive component 3, the first housing 21 can directly apply uniform axial pressure to the stationary phase 13, effectively eliminating channeling or voids that may be caused by the impact of the mobile phase, keeping the stationary phase 13 in a tight and uniform packed state, thereby significantly improving the column efficiency and separation reproducibility of the chromatographic column 1, and is particularly suitable for long-term operation or processing of complex samples.

[0037] In this embodiment, when the first housing 21 presses against the fixed phase 13, the spring 7 is compressed, thereby exposing the outlet 25 of the drain column 23 to the fixed phase 13, at which time draining can be performed. When the draining is completed, after the piston 2 rises, the first housing 21 moves down under the action of the spring 7. The first housing 21 can clean the debris on the side wall of the drain column 23, ensuring the cleanliness of the drain column 23.

[0038] In addition, during the drainage process, the first shell 21 squeezes the stationary phase 13, which in turn squeezes the drainage column 23. In this embodiment, the drainage column 23 rotates during operation. During the rotation, the stationary phase 13 can effectively prevent the outlet 25 from being blocked when stationary, thus effectively improving the drainage efficiency.

[0039] Finally, the piston 2 of the present invention is equipped with a hydraulic motor composed of hydraulic gears. The hydraulic gears are driven to rotate by high pressure fluid, and the discharge column 23 is driven to rotate by the transmission shaft 43, the first gear 41 and the second gear 42. During the rotation of the transmission shaft 43, the scraper 62 can also be driven to rotate to scrape the medicine liquid, so that the medicine liquid can flow into the discharge column 23 better and avoid excessive residue of medicine liquid.

[0040] Those skilled in the art will readily understand that the above description is merely a preferred embodiment of the present invention and is not intended to limit the present invention. Any modifications, equivalent substitutions, and improvements made within the spirit and principles of the present invention should be included within the scope of protection of the present invention.

Claims

1. A device for quantitative analysis of active pharmaceutical ingredients, characterized in that, The system includes a chromatographic column (1), which comprises a hollow column body (11). A filter screen (12) is fixedly installed at the lower end of the column body (11). A stationary phase (13) is installed above the filter screen (12). A piston (2) is installed above the stationary phase (13). The piston (2) is connected to a driving member (3) that drives it to reciprocate along the axis of the column body (11). The piston (2) includes a first housing (21) facing the stationary phase (13). The sidewall of the first housing (21) is slidably sealed to the inner wall of the column body (11). A second housing (22) is slidably installed on the side of the first housing (21) away from the stationary phase (13). An elastic support is provided between the first housing (21) and the second housing (22). Multiple connection holes are coaxially opened at the bottom of the first housing (21) and the second housing (22). A drain column (23) is provided in the connection hole. The drain column (23) is rotatably connected to the second housing (22). An inlet (24) is provided at the top of the drain column (23). An outlet (25) is provided on the bottom side wall of the drain column (23). A communication channel is provided between the outlet (25) and the inlet (24). In the natural state, the height of the outlet (25) is higher than the bottom surface height of the first housing (21). When the first housing (21) squeezes the fixed phase (13), the height of the outlet (25) is lower than the bottom surface height of the first housing (21). Multiple drain columns (23) are connected to a driving mechanism (4). The driving mechanism (4) drives the drain column (23) to rotate. The second housing (22) is connected to an inlet pipe (5) for conveying the medicine into the second housing (22).

2. The device for quantitative analysis of active pharmaceutical ingredients according to claim 1, characterized in that, The drive mechanism (4) includes a power component and a transmission component. The transmission component includes a first gear (41) that is coaxially fixedly connected to the drain column (23). Multiple first gears (41) are meshed with each other. When one of the first gears (41) rotates, it synchronously drives the other first gears (41) to rotate. One of the first gears (41) is meshed with a second gear (42). The second gear (42) is rotatably connected to the second housing (22). The second gear (42) is coaxially connected to a transmission shaft (43). The power component is connected to the transmission shaft (43) to drive it to rotate.

3. The quantitative analysis device for active pharmaceutical ingredients according to claim 2, characterized in that, The power component includes a mounting housing (44) fixedly connected to the second housing (22). The mounting housing (44) has a mounting cavity inside. A first hydraulic gear (45) and a second hydraulic gear (46) are rotatably connected in the mounting cavity. The first hydraulic gear (45) is coaxially fixedly connected to the transmission shaft (43). The mounting housing (44) is located on one side of the mounting cavity and connected to the inlet pipe (5). The other side of the mounting cavity is connected to the outlet pipe (47).

4. The device for quantitative analysis of active pharmaceutical ingredients according to claim 2, characterized in that, The second housing (22) is fixedly provided with a baffle (61) above the first gear (41) and the second gear (42). The baffle (61) and the second housing (22) form a sealed chamber. The first gear (41) and the second gear (42) are disposed in the chamber. The upper end of the drain column (23) passes through the baffle (61) and its upper end is flush with the upper plane of the baffle (61).

5. The quantitative analysis device for active pharmaceutical ingredients according to claim 4, characterized in that, The drive shaft (43) is fixedly provided with a scraper (62) above the baffle (61), and the bottom of the scraper (62) abuts against the upper surface of the baffle (61).

6. The device for quantitative analysis of active pharmaceutical ingredients according to claim 1, characterized in that, The drive unit (3) includes a hydraulic cylinder (31) consisting of a cylinder body and a hydraulic rod (32), the hydraulic rod (32) being fixedly connected to the second housing (22).

7. The device for quantitative analysis of active pharmaceutical ingredients according to claim 6, characterized in that, The hydraulic rod (32) is provided with an installation channel (33), the inlet pipe (5) is installed in the installation channel (33) and passes through the upper end of the hydraulic rod (32), and the end of the inlet pipe (5) that passes through the hydraulic rod (32) is connected to a pumping system through a hose.

8. The device for quantitative analysis of active pharmaceutical ingredients according to claim 1, characterized in that, The upper edge of the first housing (21) extends inward to form a first limiting edge (26), which is slidably connected to the second housing (22). The bottom of the second housing (22) extends outward to form a second limiting edge (27), which is slidably connected to the first housing (21).

9. The device for quantitative analysis of active pharmaceutical ingredients according to claim 8, characterized in that, The elastic support includes a spring (7), which is parallel to the axis of the second housing (22) and is disposed outside the second housing (22). A plurality of springs (7) are arranged in a circumferential array along the second housing (22). One end of the spring (7) is fixedly connected to the second housing (22) and the other end is fixedly connected to the first limiting edge (26).

10. The device for quantitative analysis of active pharmaceutical ingredients according to claim 1, characterized in that, The bottom of the column (11) is provided with a drain port (14).

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